色谱

色谱 ›› 2010, Vol. 28 ›› Issue (10): 993-996.DOI: 10.3724/SP.J.1123.2010.00993

• 技术与应用 • 上一篇    下一篇

气相色谱-质谱法测定水中痕量的四乙基铅

杨丽莉1*, 王美飞1, 李娟2, 胡恩宇1   

  1. 1. 南京市环境监测中心站, 江苏 南京 210013; 2. 江苏省环境监测中心, 江苏 南京 210024
  • 收稿日期:2010-06-17 修回日期:2010-09-14 出版日期:2010-10-28 发布日期:2010-10-28
  • 通讯作者: 杨丽莉,研究员,主要从事环境中有机污染物分析监测研究. Tel: (025)83336937, E-mail: yllyj@126.com.

Determination of tetraethyllead in water by gas chromatography-mass spectrometry

YANG Lili1*, WANG Meifei1, LI Juan2, HU Enyu1   

  1. 1. Nanjing Environment Monitoring Center, Nanjing 210013, China; 2. Jiangsu Environment Monitoring Center, Nanjing 210024, China
  • Received:2010-06-17 Revised:2010-09-14 Online:2010-10-28 Published:2010-10-28

PDF

783

被引次数

31

摘要： 建立了气相色谱-质谱(GC-MS)测定水中痕量四乙基铅的分析方法。用正己烷萃取水样中的四乙基铅,萃取液浓缩后加入同位素内标萘-d8,采用GC-MS选择离子方式(SIM)进行检测,在200 mL水样中四乙基铅的检出限可达0.04 μg/L;添加回收率为92.2%～103%,准确度好;平行5次测定的相对标准差为4.4%～13.3%。结果表明: 方法简便、快速、准确、实用,可用于水中痕量四乙基铅的测定。

关键词: 气相色谱-质谱法, 水, 四乙基铅

Abstract: A new method for the determination of tetraethyllead (TEL) in water by gas chromatography-mass spectrometry (GC-MS) has been developed. The TEL in water samples (200 mL) was extracted with hexane (50 mL) by adding 20 g NaCl, then the extracted solution was concentrated into 1.0 mL and the internal standard (naphthalene-d8) solution was added to every concentrated solution. The pretreated samples were analyzed by GC-MS. An amount of 1.0 μL solution was injected onto an HP-5ms capillary column (30 m×0.25 mm×0.25 μm) and determined by GC-MS in selected ion monitoring (SIM). The selected monitoring ions were m/z 136, 236, 237, 294 and 295. The m/z 295 was selected as quantitative ion for TEL and m/z 136 for the internal standard. The method had good linearity over the tested concentration range of 0.02~0.40 mg/L (r=0.9998) for TEL. The analytical performance characteristics of the proposed procedure were as follows: the detection limit for TEL in 200 mL water sample was 0.04 μg/L. The average recoveries and the relative standard deviations of TEL were 92.2%~103% and less than 13.3%, respectively. The method is rapid, convenient and accurate for the determination of water samples.

Key words: tetraethyllead, water, gas chromatography-mass spectrometry (GC-MS)